Method of making an adhesive and the product thereof



ILXEUTHFIBT 106- CUMPOSIHDNS, I COAHNG R PLASTIC l 1 9 Patented Oct. 9, 1934 UNITED. STATES PATENT OFFICE IMETHOD 0F MAKUQG AN ADHESIVE AND THE PRODUCT THEREOF Charles N. Cone and Harry Galber, Seattle, Wash, assignors to I. F. Laucks, Inc., Seattle, Wash, a corporation of Washington No Drawing. Application December 29, 1930,

- Serial No. 505,459

21 Claims. (01. all-'11) 0'? Our invention relates to the method of making has been used w these k199i ggy-We k an adhesive and to the product thereof. More alkali glues, but without the advantages inherparticularly, our invention will be described in Fit 1n our invention. connection with the problems arising in the art y the term fii l l lli .1-. mean or making veneer panels, but it is to be underto include the flours or meals resulting from the stood that it is not to be restricted to any such grinding 0f cakes and/0r meals remaining 811561 specific application, but is co-extensive in all 15 n r o l h n rem v m w 0 e or m fields where like problems and conditions are p rom soya beans, D fl- ,met. nuts, linseed, cottonseed, sesame seed, castor More particularly, our invention relates to the ii, m eed and other I01 seeds or class" es method f making glues or dh si having jelrepresen ed by the above named varieties. These 7 lying properties by utilizing the reactions of oil flours are all rized by having a simi seed residue flours blood, caustic alkali and forTn: larity f Composition in hat y are P 'a1de5 de d in BF Tfd FM t -m cally free from starch or contain minor per- 1 Tim of co er salts; and even the reactions of s s o s a e c ntain va yi mal blood, col m 1C a l and formaldehyde without emolmts of 21 are relatively high i ot in the addition of the oil seed residue flours. ran in from approximately 25 o epproximefil'i It is heretofore known that oil seed residue e relatively low cellulose content and e flours may be so treated as to produce jelly-like considerable content of Eeml'ceIluloses approxi- 90 glues. The process in general consists of treatf l% to 20%.

ing oil seed residue flours with caustic soda and while 111 the examples Elven m this Specificaadding forn al'dehyda tion we have used formaldehyde, we have also Such a glue was adapted to be spread on either used -W and wet or dry veneer with subsequent pressing in lime 6 W1 a Van ageu5 results and 658 25 the hot press. These jelly glues were characchem! s are nsidered as equivalents of form terized by having a high water requirement in aldehyde for our e we pwjfer m use the neighborhood of 5 part of water to one formaldehyde as it is cheap and effective. part of residue flour and this high water When we speak of blood, we mean the various requirement gave a low spread, that is a small amount of dry adhesive per unit of area glued. They are further characterized by being very free from foam and being of a jelly-like consistenc necessitating spreading by spreaders with difierent grooving irom the usual spreader which was adapted to spread glues in a liquid syl upy-like condition.

The jelly-like condition of these glues enabled them to be used on wet veneer. A syrupy Blue cannot be used on wet veneer since the liquid is readily diluted with the water of the veneer and the glue consequently becomes so thin that it is lost in the wood, due to excessive penetration; A jelly-like glue, on the other hand. is not read u without excessive penetration.

It has also been known heretofore to make adhesives using blood or b l9 c d albumin with weak alkalies. Such adhesives, while having an adva'n'tageous characteristic of functioning quickly, ha a high water requirement and consequently 105 have a concomitant drawback of a tendency to excessive penetration. Deficient glue films and starved joints are thus prone to occur to a very detrimental extent in manufacturing operations where such a, glue isemployed. Formaldehyde forms in which blood is found in commerce, such as blood albumin, dry blood or even, as noted here-' afmm w 0 products are obtained from ca tle, eep and hogs.

We have discovered that the oil seed residue jelly glues heretofore referred to may be modifled to very great advantage by the introduction of blood, either as the dry blood albumin or even as fresh blood.

When blood is admixed with the oil 5516i residue gang and the mixture is dispersed by the use or caustic soda, and jorn aldehyde, or its equivalent, E Eded, a mixture or very remarkable properties results, which properties are not predictable from the behavior of either the oil seed residue flours or the blood by themselves, or from beblood without formaldehyde.

The mixture made up as abo e described has a better spreadingconsistency than either seed residue jellies or blood jellies. Furthermore, it

It has been proposed by previous inventors toa will stay the glue nne havior of mixtures of oil seed residue flours and 106. COMPOSITIONS,

cross nererence come on PLASTiC necessary to spread, without material detriment to the strength or water resistance of the final product. Thus it will be seen that the foam is a great practical advantage. We find in this glue that we can incorporate as much as 50% by volume of foam.

As an example of the'blood-seed residue glue, we give the following formula:-

use blood by itself in jelly form or at least when thickened by the use of formaldehyde. These previous proposals, however, have produced a mixture which carried only a small amount of 5 water, hence were uneconomical to use. The preparation of these previous glues has taken a long time and hence they were not very practical for veneer glues where the glue must be made in a short time and become immediately usable. Parts Many of these proposals also use heat in the Soyg, been flour 50 preparation of the glue and it will be noted that l d albumin e 50 we avoid heat in the preparation of our improved Limp 7 glue. Caustic so 4 We have found thatblood alone, when dispersed Sodium silicate 30 16 with caustic soda, and the f grmaldehy de added Formaldehyde i realizessomei'of 'the advantage's'b'fthe mixture Water 630 of blood and seed residue flours.

Forexamplefihe fongwing formula The soya bean flour is finely ground, for example through 80 or IOU-mesh, although we do Parts 0 "mi not lnmt ourselves to this fineness. The blood n g albumin is also of about the same fineness pref- Caustic soda 4 erably. Wood flour can be incorporated to the Silicate of soda 3o extent of w1thout any impairment of Formaldehyde 1/2 strength of the glue and it thus helps to cut 25 water 650 down the spread cost. The lime can be either dry mixed with'the other ingredients or can be added as a suspension of lime and water. The four parts of caustic sodaare first put in solution in part of the water and added as a solugives a glue which in an hour or so thickens to a jelly-like consistency. We have found that mixtures of blood with strong alkalies like caustic soda or potash, and formaldehyde, have the great advantage of holding a large amount of water, and

stillretaining a spreadable consistency for a plywood glue. Weak alkalies like ammonia, etc. do not have this property. The strong alkali glues are therefore economical. In spi e of e high dilution this glue when used on plywood with hot pressing gives high adhesion and water resistance with a low spread. This is contrary to what has hitherto been thought possible in gluing plywood.

As compared with oil seed residue jelly glues of the kind heretofore known our improved oil seed residue-blood glue has the advantage of being much easier spread and enabling the panels to be removed from the press in a much quicker time. For example, with three panels of three-ply each in one opening in the hot press, we find that the bond is set so as to permit removal from the press in as short a time as two or three minutes. This could not be realized with the straight oil seed residue jelly glue. 7

We find that we can incorporate in these blood seed residue glues agvery considerable amount of foam and that this foam actually has considerable e Beneficial effect. We know that foam in previous gluing practise has been stringently avoided, so

that it has been an aim of all glue manufacturers to make glue that would be as free as possible from foam. Nevertheless, we find that when properly handled foam is not only not a detriment but can be a positise advantage. In the case of the glue under discussion we find that by incorporating a considerable amount of foam the spread is cut down, that is, it is necessary to spread less adhesive per unit of area, and that the spreading properties of the glue are improved.

In the ordinary liquid glue when foam is incorporated accidentally the spreading properties are seriously impaired, for a liquid syrupy glue when foam is incorporated with it tends to become of a consistency something like mayonnaise or whipped cream, which is very difllcult to handle on the usual glue spreader. With this combination of blood'and seed residue flours that we have discovered, however, the reverse is true. The incorporation of form actually improves the spreading properties, as well as decreasing the amount narily known as water glass. Formaldehyde is used as the ordinary io'rmaIHehyde of commerce. The lime and the silicate of soda improve the water resistance.

caustic soda may be. replaced by caustic potash. Ammonia is not, however, an e'iu'm'afit Wally different kind of a glue, the water requirement being far less and the ammonia furtheremore failing to properly disperse the seed residue part of the composition. The caustic soda or caustic potash do not need to be used as such in these glues for it appears that in this combina= tion they may be replaced by a mixture of lime "and fluoride, for example, which com5i-' natifinmixed with the glue and when freshly mixed appears to have the same effect in this composition as the use of caustic soda as such. We have not, however, kept such dry mixture in storage for any length of time to see whether it would behave in the same ways as do straight oil seed residue glues kept in storage, in which lime and a sodium salt such as sodium fluoride is mixed. For this reason we prefer to use caustic soda as such but do not limit ourselves in this application to the use of caustic as such.

In mixing the above formula, the dry mixed ingredients are first added to the water, stirred gredients, including the caustic soda, silicate and formaldehyde, are added, usually in the order named, giving glue which is ready for use immediately, the whole operation of mixing taking but from ten to twenty minutes.

This glue can be spread by the usual type at glue spreader and gives an especially strong and water resistant bond, after a very short time in the hot press; the time in the hot press varies els and the kind of wood, but when spreading this glue on dry inch birch veneer with three assemblies in one opening of a hot press the panels may be removed in from two to three minutes. The

tion. The sodium silicate is the variety ordi- In this type of glues that we have discovered, no

until thoroughly mixed, and then the liquid in- 13' scmewhat depending on the thickness of the panstrensthofthesepanelsbythelio standard plywood shear test is around 400 pounds per square inch. The water resistance, that is the strength of a test-piece after soaking it for 48 hours in water, is around 250 pounds to 300 are obtained by a spread of less than pounds of the dry glue material per thousand square feet of three-ply panel. This is a remarkably low spread when it is considered that "the usual amount of glue spread per thousand square feet of three-ply panel is from 25 to 40 pounds or more. Such adhesion results as the above are also obtained when the wet glue mixture consists of 50% or even more of foam by volume.

We have found that a further improvement can be made on glues of the type described, that is the combination of .h oodgmedlresi uefloiin with caustic soda, and fgrrnaldehyde by the addition of a small amount of copper sulphate. The addition of copper sulphate makes a further improvement in consistency, giving a jelly of a stringy character which makes it easier to spread and furthermore by the use of copper sulphate it holds this consistency for as long as three days without material change in either consistency or viscosity. This improvement in the keeping qualities is of considerable importance practically as it enables a batch of glue to be completely used up without having to throw any away.

A typical formula is as follows:

Parts Soya bean flour It will be understood that the advantages of all of the foregoing formulae are realized to a high degree in the gluing of veneer by means of hot presses.

We do not limit ourselves to the above formula: or proportions as we have found combinations with other oil seed flours and other proportions of ingredients noted and other soluble alkali metal ble alkali metal salts including trisodium phosphate, sodium carbonate, sodium silicate, sodium borate, etc, all being salts of strong bases and weak acids, which, together with hydrated lime in aqueous medium, form caustic soda. Further we have successfully used oil seed meals and blood in relative dry weight proportions ranging from 10% blood-90% oilseed Q9 11 to 100% blood -0% J oil sedfl'our, formaldehyde and caustic soda be- 1 We claim:

'-. 1. A method of making glue, which consists of treating mixtures of oil seed residue flours and blood albumin with caustic alkali in aqueous solution and adding formaldehyde.

2. A method of making glue, which consists of treating mixtures of soya bean flour and blood albumin with caustic alkali in aqueous solution and adding formaldehyde.

3. A method of making glue which consists of treating oil seed residue flours and blood albumin with hydrated lime and caustic alkali in aqueous solution and adding formaldehyde.

4. A method of making glue which consists of treating oil seed residue flours and blood alpounds per square inch. Such results as these.

salts to give excellent results, the said other solubumin with hydrated lime and caustic alkali in aqueous solution and adding formaldehyde and copper sulphate.

5. A method of making glue whichconsists of treating oil seed residue flours and blood albumin with hydrated lime and caustic alkali in aqueous solution and sodium silicate and adding formaldehyde.

6. A method of making glue, which consists of treating mixtures of oil seed residue flours and blood albumin with caustic alkali in aqueous solution and adding formaldehyde and copper sulphate.

7. A method of making glue, which consists of treating mixtures of soya bean flour and blood albumin with caustic alkali in aqueous solution and adding formaldehyde and copper sulphate.

8. A method of making glue which comprises treating blood albumen with caustic alkali in aqueous solution and formaldehyde.

9. A method of making glue which consists of treating mixtures of oil seed residue flours andblood albumin with lime and water and a salt which will produce caustic soda when mixed with lime in aqueous mixture, and formaldehyde.

10. A method of making glue which consists of treating mixtures of oil seed residue flours and blood albumin with caustic soda as such in water solution and adding formaldehyde.

11. A method of making glue which consists of treating mixtures of soya bean flour and blood albumin with caustic soda as such in water solution and adding formaldehyde.

12. An'adhesive comprising the reaction products of oil seed residue flours, blood albumin, caustic alkali in water solution and formaldehyde.

13. An adhesive comprising the reaction products of oil seed residue flours, blood albumin, caustic alkali in water solution and formaldehyde and copper sulphate.

14. An adhesive comprising the reaction products of oil seed residue flours, blood albumin, caustic alkali in water solution, hydrated lime and formaldehyde.

15. An adhesive comprising the reaction products of oil seed residue flours, blood albumin, caustic alkali in water solution, hydrated lime, formaldehyde and copper sulphate.

16. An adhesive comprising the reaction products of oil seed residue flours, blood albumin, caustic alkali, hydrated lime and sodium silicate in water solution and formaldehyde.

17. An adhesive comprising the reaction products of oilseed residue flours, blood albumin, caustic alkali, hydrated lime and sodium silicate in water solution, formaldehyde and copper sulphate.

18. An adhesive comprising the reaction products of soya bean flour, blood albumin, caustic alkali in water solution and formaldehyde.

19. An adhesive comprising the reaction products of soya bean flour, blood albumin, caustic alkali in water solution and formaldehyde and copper sulphate.

20. An adhesive comprising the reaction products of blood, caustic alkali, hydrated lime and sodium silicate in water solution together with formaldehyde.

21. An adhesive consisting of the reaction products of oil seed residue flours, blood, caustic alkali. ydrated lime and sodium silicate in water solution together with formaldehyde and copper sulphate. CHARLES N. CONE.

HARRY GALBER. 

